摘要
目的建立以氘代同位素内标测定发酵食品中氨基甲酸乙酯的GC—MS方法。方法试样中加入d5-氨基甲酸乙酯氘代同位素内标,采用Hydromatrix硅藻土吸附剂进行基质固相分散萃取,二氯甲烷洗脱浓缩后,用DB-WAX毛细管柱气相色谱分离,选择离子监测(SIM)的质谱扫描模式进行定量分析。结果方法的线性范围在10~1000μg/L,检测限(s,N≥3)为1μg/kg,定量限为10μg;不同基底样品中高低添加浓度的加标回收率为81.0-96.4%,相对标准偏差值(RSD)为2.1%~7.6%。结论该方法灵敏度高、准确度高,适合于发酵食品中氨基甲酸乙酯的常规检测。
Objective To develop a highly sensitive method for determination of ethyl carbamate in fermented foods using capillary gas chromatography with mass spectrometric detection and incorporating the use of a deuterated internal standard. Methods After addition of internal standard d5-EC,food samples were absorbed onto a column of hydromatrix diatomaceous earth and eluted with dichloromethane (DCM) then was separated by gas chromatography on a DB-WAX capillary column,identified and quantified by mass spectrometry in SIM mode. Results The correlation coefficients were good in the range of 10-1000μg/L,with a limit of detection of 1μg/kg and limit of quantity of 10μg/kg. Average recoveries of ethyl earbamate were 81.0-96.4% ,RSD were in the range of 2.1%%-7.6%. Conclusion The method is sensitive and precise for routine determination of ethyl carbamate in fermented foods.
出处
《中国热带医学》
CAS
2009年第11期2107-2108,2119,共3页
China Tropical Medicine
基金
深圳市科技计划项目(200603271)
关键词
氨基甲酸乙酯
气相色谱-质谱法
发酵食品
Ethyl carbamate
Gas chromatography-mass spectrometry(GC-MS)
Fermented foods